CN103515611A - Lithium ion positive electrode material cladded by nanometer alumina membrane and preparation method thereof - Google Patents

Lithium ion positive electrode material cladded by nanometer alumina membrane and preparation method thereof Download PDF

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CN103515611A
CN103515611A CN201210221966.9A CN201210221966A CN103515611A CN 103515611 A CN103515611 A CN 103515611A CN 201210221966 A CN201210221966 A CN 201210221966A CN 103515611 A CN103515611 A CN 103515611A
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positive electrode
solution
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preparation
electrode material
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CN103515611B (en
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马明远
王明强
程迪
徐云军
尹正中
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Henan Kelong new energy Limited by Share Ltd
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Henan Kelong Group Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention provides a lithium ion positive electrode material cladded by a nanometer alumina membrane and a preparation method thereof. The preparation method comprises the following steps: evenly mixing a positive electrode material with a deionized water solution of sodium bicarbonate; slowly adding an aluminum salt solution with a certain concentration into a mixed solution of the positive electrode material; continuously stirring at the temperature within 50 DEG C to 55 DEG C and regulating the pH value of the solution to reach 8-12 by adding a proper amount of ammonium hydroxide at the same time; stirring for 20-120 minutes; then standing for 60-100 minutes; filtering, washing and drying the solution; calcining for 2-10 hours at the temperature within 100 DEG C to 700 DEG C under the oxygen atmosphere after the drying of the solution, thereby obtaining the positive electrode material cladded by the nanometer alumina membrane, wherein the nanometer alumina membrane is within 10nm to 40nm in thickness. The method is simple in synthetic process, uniform in membrane cladding and easy in industrial production, and is used for optimizing the high-rate performance and high-temperature cycling performance of the material. Thus, the requirement of the market on the positive electrode material is satisfied well.

Description

Lithium ion anode material that a kind of nano aluminium oxide film is coated and preparation method thereof
Technical field
The invention belongs to the preparation method of cell positive material in Material Field, be specifically related to coated lithium ion anode material of a kind of nano aluminium oxide film and preparation method thereof.
Technical background
In recent years, because the fast development of IT industry improves day by day to the requirement of power supply, require that power supply is small and exquisite, the feature such as light weight, high power capacity, high cycle performance, good high-temperature behavior, high-energy-density, and lithium ion battery is widely used with its superior combination property.
In lithium ion battery, positive electrode performance quality has important impact to performance of lithium ion battery, the ternary material LiNi using at present<sub TranNum="59">x</sub>co<sub TranNum="60">y</sub>mn<sub TranNum="61">1-x-y</sub>o<sub TranNum="62">2</sub>0.4≤x≤0.9,0.1<y≤0.5th, has the transition oxide of layer structure, in charge and discharge process, have the stripping from positive pole of nickel, cobalt, manganese element, cause positive electrode degradation, show as: the problems such as capacity is low, cycle performance is bad, solution is in material, to add different units usually to improve at present, but the interpolation of these elements can make material crystal property reduce, and the efficiency for charge-discharge of material also can reduce.
Summary of the invention
Technical problem to be solved by this invention is to provide compound lithium ion positive electrode of a kind of double-coated and preparation method thereof.Under the prerequisite that does not affect positive electrode specific capacity, having overcome positive electrode is LiNi<sub TranNum="65">x</sub>co<sub TranNum="66">y</sub>mn<sub TranNum="67">1-x-y</sub>o<sub TranNum="68">2</sub>0.4≤x≤0.9, the difficult problem in the lithium ion battery field such as the efficiency for charge-discharge low and high temperature cycle performance of the material of 0.1<y≤0.5 is poor, capacity is low, cycle performance is bad, solved simultaneously positive electrode in charge and discharge process, react with electrolyte the gas that produces nowhere release can cause battery flatulence, have a strong impact on a difficult problem for capacity and the cycle performance of battery.
For solving the problems of the technologies described above, the invention provides coated lithium ion anode material of a kind of nano aluminium oxide film and preparation method thereof.
The lithium ion anode material that nano aluminium oxide film is coated, positive electrode is LiNi<sub TranNum="71">x</sub>co<sub TranNum="72">y</sub>mn<sub TranNum="73">1-x-y</sub>o<sub TranNum="74">2</sub>, 0.4≤x≤0.9,0.1<y≤0.5, the surface coated material of active substances in cathode materials is nano aluminium oxide respectively.
The preparation method of lithium ion anode material, it is characterized in that: comprise the steps:
(1) configure certain density sodium bicarbonate solution, its concentration is 0.1M-3M.
(2) positive electrode and sodium bicarbonate solution are added in reactor and stirred, with the speed of 200r/min-900r/min, stir 1-8h, temperature is at 50-55 ℃.
(3) configure certain density aluminum salt solution, its concentration is 0.01M-0.2M
(4) certain density aluminum salt solution is added in the mixed solution of positive electrode and sodium acid carbonate with 0.02L/min-0.1L/min rate of addition, stir, the pH value that simultaneously adds appropriate ammoniacal liquor regulator solution is 8-12.
(5) the middle solution of step (4) carries out static 60min-100min above, then solution is filtered, washed, and cleaning solution pH is 6.5-7.0.
(6) material after washing is carried out to suction filtration, and then in temperature, be to dry 2-20h under the condition of 60 ℃-100 ℃, after super-dry, again under oxygen atmosphere condition, calcining 2-10h just can obtain the coated positive electrode of nano aluminium oxide film.
Wherein, described aluminium source derives from AlCl 3, Al 2(SO 4) 3, AlNO 3in a kind of.
Wherein, calcining heat is at 100 ℃-700 ℃.Be preferably 400 ℃.
The lithium ion anode material that nano aluminium oxide film is coated, the average grain diameter of positive electrode is 5um-12um, is preferably 9um-12um.
Tool of the present invention has the following advantages: by regulating positive electrode and aluminium salinity can control the thickness of coating; Coating reaction is to carry out with heterogeneous Review On The Nucleation Mechanism, guarantees that first coating reaction carry out on positive electrode surface; The material of coating is to be combined in material surface with chemical bonded refractory, is difficult for making coating material to come off.Coated pellumina can form a transition zone between positive electrode and electrolyte, make lithium ion slow in active material diffusion into the surface speed, contribute to lithium ion diffusion rate in electrolyte and electrode stable, be conducive to improve the cycle performance of material, and thermal stability, the while also can be reduced the flatulence performance of battery.This method building-up process is simple, and coating is even, and nanometer film thickness is 10nm-40nm.Be easy to suitability for industrialized production, optimized high rate capability and the high temperature cyclic performance of material, met well the requirement of market to positive electrode.
Accompanying drawing explanation
Fig. 1 is for pressing the crystallogram of embodiment 1 prepared sample
Fig. 2 is for pressing the charging and discharging curve figure of embodiment 1 prepared sample
Fig. 3 is for pressing the charge and discharge cycles frequency curve figure of embodiment 1 prepared sample
Fig. 4 is for pressing the scanning electron microscope (SEM) photograph of the prepared coated rear sample of embodiment 1
Embodiment
Embodiment 1
The LiNi that is 10um by 50g average grain diameter 0.5co 0.2mn 0.3o 2positive electrode mixes with the deionized water solution that concentration is 0.3M sodium acid carbonate, then concentration, be that 0.08M liquor alumini chloridi adds in the mixed solution of positive electrode slowly, temperature is controlled at 50 ℃, and constantly stir, the pH value that simultaneously adds appropriate ammoniacal liquor regulator solution is 8.5, stir 30min, then static 60min, again solution filter, wash, at 80 ℃ of dry 6h, after super-dry again under oxygen atmosphere condition, at 400 ℃ of ℃ of calcining 6h, just can obtain the coated positive electrode of nano aluminium oxide film, this nanometer film thickness is 10nm.With this material, do positive electrode and make button cell, lithium sheet is negative pole, and discharging and recharging cut-ff voltage is 2.75v-4.25v, and 500 capacity that circulate under 2c discharging current condition are 145.4mAh/g, under 50 ℃ of conditions, 500 Capacitance reserves that circulate under 2c current condition are 143mAh/g.
Embodiment 2
The LiNi that is 10um by 50g average grain diameter 0.5co 0.2mn 0.3o 2positive electrode mixes with the deionized water solution that concentration is 1M sodium acid carbonate, then concentration, be that 0.15M aluminum sulfate solution adds in the mixed solution of positive electrode slowly, temperature is controlled at 52 ℃, and constantly stir, the pH value that simultaneously adds appropriate ammoniacal liquor regulator solution is 9, stir 30min, then static 60min, again solution filter, wash, at 80 ℃ of dry 6h, after super-dry again under oxygen atmosphere condition, at 400 ℃ of ℃ of calcining 6h, just can obtain the coated positive electrode of nano aluminium oxide film, this nanometer film thickness is 14nm.With this material, do positive electrode and make button cell, lithium sheet is negative pole, and discharging and recharging cut-ff voltage is 2.75v-4.25v, and 500 capacity that circulate under 2c discharging current condition are 147.6mAh/g, under 50 ℃ of conditions, 500 Capacitance reserves that circulate under 2c current condition are 145.1mAh/g.
Embodiment 3
The LiNi that is 10um by 50g average grain diameter 0.5co 0.2mn 0.3o 2positive electrode mixes with the deionized water solution that concentration is 1.5M sodium acid carbonate, then concentration, be that 0.2M liquor alumini chloridi adds in the mixed solution of positive electrode slowly, temperature is controlled at 50 ℃, and constantly stir, the pH value that simultaneously adds appropriate ammoniacal liquor regulator solution is 9.5, stir 30min, then static 60min, again solution filter, wash, at 80 ℃ of dry 6h, after super-dry again under oxygen atmosphere condition, at 500 ℃ of ℃ of calcining 6h, just can obtain the coated positive electrode of nano aluminium oxide film, this nanometer film thickness is 20nm.With this material, do positive electrode and make button cell, lithium sheet is negative pole, and discharging and recharging cut-ff voltage is 2.75v-4.25v, and 500 capacity that circulate under 2c discharging current condition are 148.3mAh/g, under 50 ℃ of conditions, 500 Capacitance reserves that circulate under 2c current condition are 144.2mAh/g.
Comparative example
By not doing positive electrode through the material of alumina-coated, make button battery, lithium sheet is negative pole, discharging and recharging cut-ff voltage is 2.75v-4.25v, 500 capacity that circulate under 2c discharging current condition are 135.3mAh/g, under 50 ℃ of conditions, 500 Capacitance reserves that circulate under 2c current condition are 127.2Ah/g.

Claims (6)

1. the coated lithium ion anode material of nano aluminium oxide film, is characterized in that: positive electrode is LiNi<sub TranNum="120">x</sub>co<sub TranNum="121">y</sub>mn<sub TranNum="122">1-x-y</sub>o<sub TranNum="123">2</sub>, 0.4≤x≤0.9,0.1<y≤0.5, the surface coated material of positive electrode is nano aluminium oxide.
2. the preparation method of the lithium ion anode material of a kind of double-coated according to claim 1, is characterized in that: comprise the steps:
(1) sodium bicarbonate solution that configuration concentration is 0.1M-3M;
(2) positive electrode and sodium bicarbonate solution are added in reactor and stirred;
(3) aluminum salt solution that configuration concentration is 0.01M-0.2M;
(4) aluminum salt solution is added in the mixed solution of positive electrode and sodium acid carbonate, stir, the pH value that simultaneously adds appropriate ammoniacal liquor regulator solution is 8-12.
(5) solution in step (4) is carried out static, then solution is filtered, washed, cleaning solution pH is 6.5-7.0.
(6) material after washing is carried out to suction filtration, dry, calcining, obtains the coated positive electrode of nano aluminium oxide film.
3. preparation method according to claim 2, is characterized in that:
In step (2), with the speed of 200r/min-900r/min, instead in answering still, stir 1-8h, temperature is at 50-55 ℃;
In step (4), aluminum salt solution is added in the mixed solution of positive electrode and sodium acid carbonate with 0.02L/min-0.1L/min rate of addition;
In step (5), solution in step (4) is carried out to static 60min-100min;
In step (6), the material after washing is carried out to suction filtration, and then in temperature, be to dry 2-20h under the condition of 60 ℃-100 ℃, after super-dry, then under oxygen atmosphere condition, calcining heat is at 100 ℃-700 ℃, calcining 2-10h, just can obtain the coated positive electrode of nano aluminium oxide film.
4. according to the preparation method described in claim 2 or 3, it is characterized in that: described aluminium source derives from AlCl 3, Al 2(SO 4) 3, AlNO 3in a kind of.
5. preparation method according to claim 3, is characterized in that: calcining heat is 400 ℃.
6. the coated lithium ion anode material of a kind of nano aluminium oxide film according to claim 1, is characterized in that: the average grain diameter of positive electrode is 5um-12um; Be preferably 9um-12um.
CN201210221966.9A 2012-06-29 2012-06-29 A kind of lithium ion anode material of nano oxidized aluminium film cladding and preparation method thereof Active CN103515611B (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103794779A (en) * 2014-02-27 2014-05-14 广西师范大学 Aluminum oxide coated lithium manganese oxide spinel positive electrode material as well as preparation method thereof
CN104766960A (en) * 2015-04-13 2015-07-08 河北工业大学 Method for modifying lithium nickel manganese oxide positive electrode material for lithium ion battery
JP2017134997A (en) * 2016-01-27 2017-08-03 日立マクセル株式会社 Nonaqueous electrolyte secondary battery
CN108091927A (en) * 2017-12-13 2018-05-29 桑顿新能源科技有限公司 A kind of lithium ion battery and preparation method thereof of high safety, long circulation life
CN108666534A (en) * 2017-03-27 2018-10-16 天津国安盟固利新材料科技股份有限公司 A kind of anode material for lithium-ion batteries of double-coating and preparation method thereof
CN108987681A (en) * 2017-06-01 2018-12-11 中天新兴材料有限公司 Ternary composite cathode material, preparation method and the lithium battery using it
WO2024008000A1 (en) * 2022-07-04 2024-01-11 蔚来电池科技(安徽)有限公司 Secondary battery and apparatus

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Publication number Priority date Publication date Assignee Title
CN1595689A (en) * 2003-09-08 2005-03-16 中国科学院物理研究所 Positive electrode material of manganese series, and preparation and usage thereof
CN1945876A (en) * 2006-10-26 2007-04-11 清华大学 Method for preparing lithium ion battery positive electrode composite material
CN101764210A (en) * 2010-01-14 2010-06-30 镇江科捷锂电池有限公司 Anode material of lithium battery in Al2O3 wrapping manganese-base layered crystal structure

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1595689A (en) * 2003-09-08 2005-03-16 中国科学院物理研究所 Positive electrode material of manganese series, and preparation and usage thereof
CN1945876A (en) * 2006-10-26 2007-04-11 清华大学 Method for preparing lithium ion battery positive electrode composite material
CN101764210A (en) * 2010-01-14 2010-06-30 镇江科捷锂电池有限公司 Anode material of lithium battery in Al2O3 wrapping manganese-base layered crystal structure

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103794779A (en) * 2014-02-27 2014-05-14 广西师范大学 Aluminum oxide coated lithium manganese oxide spinel positive electrode material as well as preparation method thereof
CN104766960A (en) * 2015-04-13 2015-07-08 河北工业大学 Method for modifying lithium nickel manganese oxide positive electrode material for lithium ion battery
CN104766960B (en) * 2015-04-13 2017-01-18 河北工业大学 Method for modifying lithium nickel manganese oxide positive electrode material for lithium ion battery
JP2017134997A (en) * 2016-01-27 2017-08-03 日立マクセル株式会社 Nonaqueous electrolyte secondary battery
CN108666534A (en) * 2017-03-27 2018-10-16 天津国安盟固利新材料科技股份有限公司 A kind of anode material for lithium-ion batteries of double-coating and preparation method thereof
CN108666534B (en) * 2017-03-27 2021-03-19 天津国安盟固利新材料科技股份有限公司 Double-layer coated lithium ion battery anode material and preparation method thereof
CN108987681A (en) * 2017-06-01 2018-12-11 中天新兴材料有限公司 Ternary composite cathode material, preparation method and the lithium battery using it
CN108091927A (en) * 2017-12-13 2018-05-29 桑顿新能源科技有限公司 A kind of lithium ion battery and preparation method thereof of high safety, long circulation life
WO2024008000A1 (en) * 2022-07-04 2024-01-11 蔚来电池科技(安徽)有限公司 Secondary battery and apparatus

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